CN108333137B - Method for measuring generation performance of ammonia product of three-way catalytic material - Google Patents
Method for measuring generation performance of ammonia product of three-way catalytic material Download PDFInfo
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 115
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 58
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 36
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 238000012360 testing method Methods 0.000 claims abstract description 33
- 239000012298 atmosphere Substances 0.000 claims abstract description 31
- 238000006555 catalytic reaction Methods 0.000 claims abstract description 8
- 239000007789 gas Substances 0.000 claims description 41
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 14
- 238000012937 correction Methods 0.000 claims description 13
- 238000001514 detection method Methods 0.000 claims description 13
- 239000012495 reaction gas Substances 0.000 claims description 11
- 239000004215 Carbon black (E152) Substances 0.000 claims description 7
- 229930195733 hydrocarbon Natural products 0.000 claims description 7
- 150000002430 hydrocarbons Chemical class 0.000 claims description 7
- 238000004364 calculation method Methods 0.000 claims description 6
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 claims description 5
- 238000002485 combustion reaction Methods 0.000 claims description 5
- 238000004519 manufacturing process Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 claims description 3
- 238000000576 coating method Methods 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims 3
- 230000035484 reaction time Effects 0.000 claims 2
- 125000004122 cyclic group Chemical group 0.000 claims 1
- 230000001105 regulatory effect Effects 0.000 claims 1
- 239000004576 sand Substances 0.000 claims 1
- 230000001360 synchronised effect Effects 0.000 claims 1
- 238000011056 performance test Methods 0.000 abstract description 10
- 239000003054 catalyst Substances 0.000 abstract description 9
- 239000003344 environmental pollutant Substances 0.000 abstract description 3
- 231100000719 pollutant Toxicity 0.000 abstract description 3
- 230000007246 mechanism Effects 0.000 abstract description 2
- 238000011160 research Methods 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 abstract 1
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 10
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 7
- 230000015572 biosynthetic process Effects 0.000 description 7
- 239000006004 Quartz sand Substances 0.000 description 5
- 229910052763 palladium Inorganic materials 0.000 description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 229920000742 Cotton Polymers 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000007689 inspection Methods 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 150000001768 cations Chemical class 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- 239000012299 nitrogen atmosphere Substances 0.000 description 2
- 239000010453 quartz Substances 0.000 description 2
- 229910052703 rhodium Inorganic materials 0.000 description 2
- 239000010948 rhodium Substances 0.000 description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- 238000012935 Averaging Methods 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000012216 screening Methods 0.000 description 1
- 239000011163 secondary particle Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01M—TESTING STATIC OR DYNAMIC BALANCE OF MACHINES OR STRUCTURES; TESTING OF STRUCTURES OR APPARATUS, NOT OTHERWISE PROVIDED FOR
- G01M3/00—Investigating fluid-tightness of structures
- G01M3/02—Investigating fluid-tightness of structures by using fluid or vacuum
- G01M3/26—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors
- G01M3/32—Investigating fluid-tightness of structures by using fluid or vacuum by measuring rate of loss or gain of fluid, e.g. by pressure-responsive devices, by flow detectors for containers, e.g. radiators
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N2021/3595—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using FTIR
Abstract
The invention discloses a method for measuring the generation performance of a three-way catalytic material ammonia product, which is a method for realizing the generation performance test of the three-way catalytic material ammonia product on a fixed bed catalytic reaction device, can realize the accurate measurement of the ammonia selectivity and the ammonia generation rate in the three-way catalytic reaction through the specific time sequence control of the gas distribution atmosphere of a chemical reaction, has the advantages of rapidness, accuracy, reliability and the like, and can provide technical support for the research on the generation mechanism and emission control of ammonia pollutants in a three-way catalyst. The method for determining the generation performance of the ammonia product of the three-way catalytic material comprises the following steps: (1) preparing and pretreating a sample; (2) calibrating a gas analyzer; (3) testing the air tightness of the fixed bed catalytic reaction device; (4) the ammonia selectivity and the ammonia generation rate are measured, and the cycle switching frequency of the chemical reaction for distributing rich-burn/lean-burn atmosphere is not less than 5 times.
Description
Technical Field
The invention relates to a performance evaluation test method of an automobile three-way catalytic material, in particular to a method for realizing the performance test of ammonia product generation by the three-way catalytic material on a fixed bed catalytic reaction device.
Background
In order to meet the increasingly strict requirements of emission limits of carbon monoxide (CO) and Hydrocarbon (HC) of light gasoline vehicles, the consumption of noble metal palladium in the three-way catalyst for tail gas purification is greatly increased, so that the emission of ammonia is high after the three-way catalyst is installed, and the emitted ammonia becomes a main cation (NH) forming secondary particles4 +) Source, severe shadowAnd the environment is loud. The three-way catalyst is used as a key part for controlling the pollution emission of light gasoline vehicles, is the most main automobile part unit causing the emission of ammonia pollutants, and has the core of three-way catalytic material, and the emission of ammonia depends on the composition of the three-way catalytic material and the transient working condition characteristics of an engine.
The ammonia emission of the light gasoline vehicle is mainly focused on a temperature window of 300-600 ℃ after cold start, and at present, an ammonia emission test method in the whole vehicle emission process is relatively mature, however, an ammonia product generation performance test method of a three-way catalytic material is not reported or disclosed, so that research work for effectively controlling ammonia emission from the perspective of the catalytic material is restricted, and more mechanisms related to generation of ammonia pollutants in a three-way catalytic converter are only guessed. In order to develop a three-way catalytic material capable of effectively controlling ammonia emission as soon as possible, a rapid, accurate and reliable method for testing the generation performance of an ammonia product of the three-way catalytic material is urgently needed to be developed by combining the emission characteristics of automobile exhaust.
Disclosure of Invention
The invention aims to provide a rapid, accurate and reliable method for testing the generation performance of a three-way catalytic material ammonia product, which is used for measuring the ammonia selectivity and the ammonia generation rate of a catalytic material in a dynamic catalytic reaction process at a constant temperature, optimizing the composition and the structure of the three-way catalytic material according to the indexes and realizing the effective control of ammonia emission from the perspective of the catalytic material. The invention discloses a test method for determining the generation performance of a three-way catalytic material ammonia product, which mainly utilizes a fixed bed catalytic reaction device and a Fourier transform infrared multi-component gas analyzer for gas component online detection and is characterized by testing two performance indexes of ammonia selectivity and ammonia generation rate of the three-way catalytic material.
The method for testing the generation performance of the ammonia product comprises the following specific steps:
(1) test sample preparation
Weighing 5-10 g of a powder sample to be tested, putting the powder sample into a die of a tablet press, performing tabletting molding under the pressure condition of 15MPa, crushing and grinding the powder sample by using an agate mortar, and screening out at least 2 g of the sample to be tested with 40-60 meshes by using a 40-mesh and 60-mesh standard sieve for testing the generation performance of the ammonia product.
(2) Pretreatment of test samples
And drying the screened sample to be tested with 40-60 meshes in a vacuum drying oven, vacuumizing, heating to 80 ℃, and keeping the temperature for 30 minutes.
Weighing 0.1-1.0 g of a sample to be tested after vacuum drying, and recording the accurate mass m of the weighed samplecat.And the numerical value is accurate to 0.0001g, simultaneously weighing 60-mesh quartz sand with the same mass, and uniformly mixing the quartz sand and the quartz sand.
The inner wall of the fixed bed catalytic reactor is wiped clean by alcohol cotton, a proper amount of quartz cotton is inserted, the amount of the quartz cotton depends on the structure of the reactor, but the thermocouple for detecting the reaction temperature is required to detect the temperature of the surface of the catalyst sample, the uniformly mixed test sample-quartz sand mixture is filled, and the reactor is sealed.
At 1% O2+N2Heating to 500 deg.C at a rate of 10 deg.C/min under (balance gas) atmosphere, holding the temperature for 30 min, and then heating in N2And (4) cooling or heating to the ammonia product generation performance test temperature under the atmosphere condition, thus finishing the pretreatment process of the test sample.
(3) Calibration of an analyzer
After the Fourier transform infrared multi-component gas analyzer for gas component online detection is stable in starting state (special attention needs to be paid to the stable condition of the gas cell pressure of the analyzer), NO and NO are adopted2And NH3Standard gas to NO and NO of analyzer respectively2And NH3Calibrating the component detection values, NO and NH3The concentration of standard gas is close to 500ppm, NO2The concentration of the standard gas does not exceed 100ppm, and the air inlet pressure and the total volume flow of the standard gas are required to be completely consistent with the actual test conditions.
Stabilizing for at least 10 min after introducing standard gas, detecting a concentration value every 5s, with the concentration detection value not less than 100, averaging 100 detection values, and recording as C2。
The concentration of standard gas C1And the detection value C of the analyzer2The ratio of (A) to (B) is used as a concentration correction factor ζ, NO2And NH3The concentration correction coefficients of the components are respectively recorded as ζ1、ζ2And ζ3NO, NO in the process of testing the ammonia product generation performance2And NH3And multiplying the detection value of the analyzer of the component by the corresponding correction coefficient to realize the correction of the concentration detection value.
(4) Device air tightness inspection
The fixed bed catalytic reaction device airtightness inspection is to close the valve at the air outlet of the device, introduce 0.3MPa nitrogen, balance for at least 10 minutes, close the valve at the air inlet, and read the pressure gauge readings.
And reading the readings of the pressure gauge again after 5 minutes, if the pressure attenuation rate is not lower than 5 percent, determining that the air tightness is good, otherwise, checking all air path connecting ports of the device until the air tightness is checked to pass.
(5) Constant temperature dynamic test
After the gas tightness inspection is passed, keeping the reaction temperature constant, introducing a lean-burn atmosphere reaction gas, adjusting the pressure of all gas inlets to be 0.1MPa, and adopting an analyzer sampling mode of 'catalyst rear end', namely detecting the gas component change after the reaction on line and collecting a concentration value every 1 s.
The lean-burn reaction atmosphere is as follows: 1000ppm CO +3000ppm HC +500ppm NO + 8% H2O+8％CO2+N2(balance gas) + O2(greater than 4750 ppm).
The total volume flow of reaction gas is determined according to the airspeed condition by coating 200 g of three-effect catalytic coating material on each liter of honeycomb carrier, and the reaction airspeed is 20000-120000 h-1And determining the flow value of each gas path according to the total gas volume flow, the test concentration condition and the concentration of each gas cylinder.
As shown in the attached figure 1, the rich-burn/lean-burn reaction atmosphere is switched circularly, the total time of single circular switching is 60-300 s, the duration time of the lean-burn condition is longer than that of the rich-burn condition, the number of times of circular switching is not less than 5 times, and the reaction test temperature is a specific constant temperature within the temperature range of 250-600 ℃.
The rich combustion reaction atmosphere is as follows: 1000ppm CO +3000ppm HC +500ppm NO + 8% H2O+8％CO2+N2(Balancing)Gas) + O2(less than 4750 ppm).
The adjusting range of the rich/lean atmosphere conditions is as follows: the oxygen excess coefficient lambda is 0.95 to 1.05.
And switching the sampling mode of the analyzer to be a catalyst front end, namely detecting the gas component change before reaction on line, collecting a concentration value every 1s, keeping the reaction test temperature and the cycle switching condition of the rich-burn/lean-burn reaction atmosphere unchanged, and switching to be a nitrogen atmosphere after the cycle switching times exceed 5 times to finish the ammonia product generation performance test.
(6) Calculation of NOx conversion
NO and NO2Multiplying the detected values of the analyzer by the corresponding correction coefficients ζ1And ζ2Respectively obtaining NO and NO2Correcting the concentration of the components, and adding NO and NO at the same time2And adding the corrected values of the component concentrations to obtain the NOx concentration.
Integrating the function f (t) of the NOx concentration at the front end of the catalytic material with respect to time, and recording the integral value A1(FIG. 2 a).
That is to say that the first and second electrodes,
tnthe time taken for the nth rich/lean reaction atmosphere cycle to switch over (as shown in fig. 2) is expressed in s.
The function g (t) of the NOx concentration at the rear end of the catalytic material with respect to time is integrated over time, and the integrated value is recorded as A2(FIG. 2 b).
That is to say that the first and second electrodes,
according to the formula
The NOx conversion χ was calculated.
(7) Calculation of Ammonia Selectivity and Ammonia Generation Rate
NH3Component analyzer detection value multiplied by its correction coefficient ζ3Obtaining NH3Correction of the concentration of the component.
Catalytic material rear end NH3The concentration correction values of the components are integrated over time as a function h (t) of time, the integral value being denoted A3(FIG. 3).
That is to say that the first and second electrodes,
according to the formula
The ammonia selectivity S was calculated.
According to the formula
The ammonia production rate R is calculated.
In the formula, V is the total volume flow of the reaction gas, and the unit is mL/min; m iscat.The actual loading mass of the catalytic material is given in g.
Drawings
FIG. 1 is a timing diagram of the atmosphere control of chemical reaction according to the present invention
FIG. 2 is a schematic of the pre-reaction NOx (FIG. 2a), post-reaction NOx (FIG. 2b) concentration curve integral calculations and the calculation of reaction-participating NOx (FIG. 2c) of the present invention
FIG. 3 shows NH of the present invention3Generating a concentration curve definite integral calculation diagram
FIG. 4 is a graph comparing the results of ammonia product formation performance tests of a palladium-only three-way catalytic material at a reaction temperature of 450 ℃ under conditions of a single rich/lean reaction atmosphere cycle (150s) in which the duration of the rich atmosphere is 15s (FIG. 4a), 30s (FIG. 4b), and 45s (FIG. 4c), respectively
FIG. 5 is a graph comparing the results of the ammonia product formation performance test of the bimetallic three-way catalyst material of palladium and rhodium under the circulating conditions of rich (30 s)/lean (120s) reaction atmosphere at the reaction temperatures of 350 deg.C (FIG. 5a), 450 deg.C (FIG. 5b) and 550 deg.C (FIG. 5 c).
Detailed Description
In order to more clearly state the technical means and the creative characteristics of the implementation of the invention, the invention is further illustrated by combining the test examples of the ammonia product generation performance of different three-way catalytic materials and the attached drawings:
preparing a 40-60-mesh granular sample by using a tablet press, a mortar and a standard sieve, drying in vacuum, weighing 0.1-1.0 g of the granular sample by using an electronic balance, accurately recording the mass of the sample, and accurately measuring the numerical value to 0.0001 g.
Uniformly mixing the weighed sample with 60-mesh quartz sand with the same mass, and then putting the mixture into a fixed bed reactor for pretreatment, wherein the pretreatment conditions are as follows: the treatment atmosphere was 1% O2+N2And (balance gas), wherein the pretreatment temperature is 500 ℃, the pretreatment time is 30 minutes, and then the temperature is reduced or increased to the test temperature in the nitrogen atmosphere.
And (5) carrying out air tightness test on the fixed bed reaction device.
After the air tightness test is passed, carrying out chemical reaction atmosphere control (the oxygen excess coefficient lambda is controlled within the range of 0.95-1.05) according to a timing diagram shown in the attached drawing 1, starting an ammonia product generation performance test, wherein the total time of single cycle switching is 60-300 s, the duration time of a lean burn condition is longer than that of a rich burn condition, and the cycle switching frequency is not less than 5 times.
According to the formula
the NOx conversion, ammonia selectivity and ammonia formation rate were calculated separately.
In the formula (I), the compound is shown in the specification,
and
all adopt Origin data processing software to calculate (figure 2,Figure 3) comprises the following specific steps: from 0 to t is selectednArea → Analysis → Ingetrate, click on the "OK" button to get the "area" value, i.e. the constant integration value.
Example 1 a palladium-only three-way catalyst material was selected to perform ammonia product formation performance testing under rich gas atmosphere conditions of λ 0.98 and lean gas atmosphere conditions of λ 1.02, at a test temperature of 450 ℃ and a volume space velocity of SV＝60000h-1The total time for switching of the single cycle was 150s, wherein the duration of the rich atmosphere condition was 15s, 30s and 45s, respectively, corresponding to the test results of fig. 4a, 4b and 4c, respectively.
Table 1 the results of the ammonia product formation performance tests for different durations of the rich atmosphere conditions are shown in table 1.
Comparison of Ammonia product Generation Performance for Rich gas atmosphere conditions duration of 15s, 30s and 45s
Attached table 1
Example 2a palladium and rhodium three-way catalytic material was selected for ammonia product formation performance testing, with rich gas atmosphere conditions of λ 0.98, lean gas atmosphere conditions of λ 1.02, rich gas atmosphere conditions duration of 30S, rich gas atmosphere conditions duration of 120S, and volume space velocity of S in a single cycleV＝60000h -1350 ℃, 450 ℃ and 550 ℃ are respectively selected as the test temperature, and the corresponding test results are respectively shown in figure 5a, figure 5b and figure 5 c.
The results of the ammonia product formation performance tests at different test temperatures are shown in the attached table 2.
FIG. 2 is a graph showing comparison of the ammonia production performance at 350 ℃, 450 ℃ and 550 ℃ in the test
Attached table 2
Claims (1)
1. Three-effect catalytic material ammonia product generationThe method for testing the performance is characterized in that: the method is realized on a fixed bed catalytic reaction device, under the constant reaction temperature within the temperature range of 250-600 ℃, the rich-burn/lean-burn atmosphere conditions of chemical reaction gas distribution are circularly switched, and a Fourier transform infrared multi-component gas analyzer respectively detects NO and NO in the reaction gas at the front end and the reaction gas at the rear end of the catalytic material2And NH3Generating component concentration change, collecting experimental data, obtaining the integral area of the concentration curve to time by adopting Origin data processing software, and obtaining the concentration curve through a formula:
separately calculating nitrogen oxides NOx, i.e. NO and NO2Conversion of the sum ofχSelectivity of ammoniaSAnd the rate of production of ammonia R,
wherein the ammonia production rate is expressed in units of μ g [ NH ]3]/(s·gcat.)；A 1、A 2AndA 3respectively catalyzing front NOx, back NOx and reacting to generate NH3Component concentration (ppm) functionf(t)、g(t) Andh(t) For reaction time 0 tot nConstant integral value of 1.285 × 10−5Is a correlation coefficient;Vthe total volume flow of the reaction gas is in mL/min;t nis as followsnThe time for finishing the cyclic switching of the rich-burn/lean-burn reaction atmosphere is s;m cat.the actual loading mass of the catalytic material, in g,
the dynamic test is carried out at a constant temperature within the temperature range of 250-600 ℃, the chemical reaction gas distribution carries out rich combustion/lean combustion atmosphere cycle switching, the total time of single cycle switching is 60-300 s, the duration time of the lean combustion condition is longer than that of the rich combustion condition, the cycle switching frequency is not less than 5 times,
by C3H6Or C3H8The method is used for preparing 1000ppm CO +3000ppm HC +500ppm NO + 8% H by regulating chemical reaction instead of Hydrocarbon (HC) component in gasoline vehicle exhaust2O +8% CO2+ N2(balance gas) + O2O in (concentration to be determined)2Content, the rich-burn/lean-burn atmosphere condition adjustment of reaction gas distribution is realized, and the adjustment range is as follows: coefficient of excess oxygenλ=0.95~1.05,
The actual loading amount of the catalytic material is 0.1-1.0 g, the total volume flow of the reaction gas is determined according to the condition of the space velocity calculated according to the three-effect catalytic coating material of 200 g coated on each liter of honeycomb carrier, and the reaction space velocity is 20000-120000 h−1,
On-line synchronous analysis of NO and NO in reaction gas by Fourier transform infrared multi-component gas analyzer2And NH3Composition, collecting concentration data every 1s, and comparing NO and NO at the same time point2The corrected concentration detection value is added as the NOx concentration value at the time point,
by using NO, NO2And NH3The standard gas is used for calibrating the Fourier transform infrared multi-component gas analyzer, the requirements of the air inlet pressure and the total volume flow of the standard gas are completely consistent with the actual test conditions, the pressure of a gas cell of the analyzer is kept constant, and NO and NH are added3The concentration of standard gas is close to 500ppm, NO2The concentration of the standard gas is not more than 100ppm, and the concentration of the standard gas is measuredC 1And the detection value of the analyzerC 2The ratio of (A) to (B) is used as a concentration correction factor ζ, NO2And NH3The concentration correction coefficients of the components are respectively recorded as ζ1、ζ2And ζ3NO, NO in the process of testing the ammonia product generation performance2And NH3The detection value of the analyzer of the component is multiplied by the corresponding correction coefficient, so that the correction of the concentration detection value is realized,
the catalytic material is required to be tested before the ammonia generation performance is testedPerforming pretreatment under 1% O2+ N2(balance gas), pretreatment temperature 500 ℃, pretreatment time 30 minutes, and under N2Raising the temperature or reducing the temperature to the testing temperature in the atmosphere,
NOx concentration value, NH, of front and rear ends of catalytic material3The concentration correction values are plotted against the reaction time and are each plotted as a function of concentrationf(t)、g(t) Andh(t) To indicate that the user is not in a normal position,
pairing functions with Origin data processing softwaref(t)、g(t) Andh(t) Within 0 tot nPerforming constant integral calculation, wherein the constant integral values are respectivelyA 1、A 2AndA 3the method comprises the following specific steps: is selected from 0 tot nRegion → Analysis → ingerate, the value of "area" obtained by clicking the "OK" button is a constant integral value, and the NOx conversion rate, ammonia selectivity and ammonia production rate are calculated according to the formulas (1), (2) and (3).
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| CN111983132A (en) * | 2020-08-14 | 2020-11-24 | 昆明贵研催化剂有限责任公司 | Small sample evaluation method for performance of three-way catalyst |
| CN117181237A (en) * | 2023-01-13 | 2023-12-08 | 昆明贵研催化剂有限责任公司 | Catalyst for preparing ammonia by using waste gas containing CO and NOx, preparation method and ammonia preparation method |
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